CN109554762A - A kind of polysilicon etch solution additive and its application - Google Patents
A kind of polysilicon etch solution additive and its application Download PDFInfo
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- CN109554762A CN109554762A CN201811547982.0A CN201811547982A CN109554762A CN 109554762 A CN109554762 A CN 109554762A CN 201811547982 A CN201811547982 A CN 201811547982A CN 109554762 A CN109554762 A CN 109554762A
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- additive
- polysilicon
- etching
- water
- basal liquid
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 37
- 239000000654 additive Substances 0.000 title claims abstract description 35
- 230000000996 additive effect Effects 0.000 title claims abstract description 35
- 229920005591 polysilicon Polymers 0.000 title claims abstract description 35
- 238000005530 etching Methods 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 17
- 239000010703 silicon Substances 0.000 claims abstract description 17
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 12
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 12
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 10
- 239000008103 glucose Substances 0.000 claims abstract description 10
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims abstract description 9
- CYDQOEWLBCCFJZ-UHFFFAOYSA-N 4-(4-fluorophenyl)oxane-4-carboxylic acid Chemical compound C=1C=C(F)C=CC=1C1(C(=O)O)CCOCC1 CYDQOEWLBCCFJZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229930003268 Vitamin C Natural products 0.000 claims abstract description 9
- 229940005581 sodium lactate Drugs 0.000 claims abstract description 9
- 235000011088 sodium lactate Nutrition 0.000 claims abstract description 9
- 239000001540 sodium lactate Substances 0.000 claims abstract description 9
- 235000019154 vitamin C Nutrition 0.000 claims abstract description 9
- 239000011718 vitamin C Substances 0.000 claims abstract description 9
- MPPQGYCZBNURDG-UHFFFAOYSA-N 2-propionyl-6-dimethylaminonaphthalene Chemical compound C1=C(N(C)C)C=CC2=CC(C(=O)CC)=CC=C21 MPPQGYCZBNURDG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 6
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 3
- 229960001031 glucose Drugs 0.000 claims abstract description 3
- 235000001727 glucose Nutrition 0.000 claims abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 3
- 239000001257 hydrogen Substances 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 19
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 18
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 2
- 239000006071 cream Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 210000002268 wool Anatomy 0.000 abstract description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- ZHPNWZCWUUJAJC-UHFFFAOYSA-N fluorosilicon Chemical compound [Si]F ZHPNWZCWUUJAJC-UHFFFAOYSA-N 0.000 description 3
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 3
- 238000005266 casting Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30604—Chemical etching
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Weting (AREA)
Abstract
The invention proposes a kind of polysilicon etch solution additive and its applications, additive includes ethylene glycol monobutyl ether, glucose, sodium lactate, vitamin C, polyethylene glycol, prodan and water, additive package each component simultaneously controls temperature and flows back under conditions of 120-130 DEG C about 10 hours, obtain additive, additive and basic acid solution are mixed to get etching solution, when carrying out surface wool manufacturing etching to polysilicon chip using etching solution of the invention, the bubble hydrogen of generation is very tiny, and it can quickly leave the interface of silicon wafer, so as to so that the etching of silicon chip surface is more uniform, the Reducing thickness of polysilicon chip also can control again in lesser range simultaneously.
Description
Technical field
The present invention relates to photovoltaic material preparation technical field more particularly to a kind of polysilicon etch solution additive and its answer
With.
Background technique
The extensive key using solar power generation is to prepare low cost, efficient solar battery.The drawing of monocrystalline silicon
Stick complex process, and silicon material higher cost；And the casting ingot process of polysilicon is simple, and the utilization rate of rectangular ingot casting silicon material is higher,
Production cost can be significantly reduced, 98% or more photovoltaic cell is polysilicon solar cell on international market at present.
However monocrystalline silicon suede anti-reflection effect is substantially better than polysilicon, the uniform monocrystalline silicon of crystalline phase distribution passes through anisotropy
Caustic corrosion can obtain uniformly intensive pyramid micro-structure, it can be achieved that 10% average reflectance below；And inside polysilicon
There are crystal boundaries, using acid corrosion method used obtained flannelette average reflectance 20% or more, to influence mentioning for battery whole efficiency
It rises.
For polysilicon, it is desirable to reduce average reflectance, then need to improve the flannelette pattern of polysilicon,
Ask polysilicon surface that can uniformly, comprehensively cover layer of surface micro-structure, next needs to improve the surface quality of flannelette, reduces
Crackle, distortion of lattice or the sub-surface damage of silicon chip surface.
Summary of the invention
In view of this, the invention proposes one kind can reduce silicon chip surface Reducing thickness, keep silicon chip surface corrosion more equal
Even polysilicon etching carves solution additive and its application.
The technical scheme of the present invention is realized as follows: the present invention provides a kind of polysilicon etch solution additive and its answering
With, including ethylene glycol monoethyl ether, glucose, sodium lactate, vitamin C, polyethylene glycol, prodan and water.
On the basis of above technical scheme, it is preferred that be by mass percentage 100% meter, the ethylene glycol monobutyl ether is
0.5-2%, the glucose are 1.5-3%, and the sodium lactate is 1-1.5%, and the vitamin C is 0.2-0.6%, described poly-
Ethylene glycol is 1-4%, and the prodan is 0.1-0.8%, and surplus is water.
On the basis of above technical scheme, it is preferred that the water is deionized water.
On the basis of above technical scheme, it is preferred that the molecular weight of the polyethylene glycol is 500-2000.
Another technical solution of the invention is the etching solution using above-mentioned additive, including polysilicon etch solution additive and
The mass ratio of basal liquid, the polysilicon etch solution additive and basal liquid is (1.5-5): 100.
On the basis of above technical scheme, it is preferred that the basal liquid includes hydrofluoric acid, nitric acid and water, the hydrogen fluorine
Acid: nitric acid: the volume ratio of water is 1: (5-7): (2-4).
Still more preferably, the mass concentration of the hydrofluoric acid is 40%, and the mass concentration of the nitric acid is 50%.
The present invention also provides more than one to state the method that additive is etched, comprising the following steps:
S1, it is by mass percentage 100% meter, mixes 0.5-2% ethylene glycol monobutyl ether, 1.5-3% glucose, 1-
1.5% sodium lactate, 0.2-0.6% vitamin C, 1-4% polyethylene glycol, 0.1-0.8% prodan and surplus water, control temperature
120-130 DEG C of back flow reaction 8-12h is spent, additive is obtained；
S2, be by volume 1: (5-7): (2-4) measures hydrofluoric acid, nitric acid and water, is mixed evenly, obtains basis
Liquid；
S3, control basal liquid temperature are at 6-9 DEG C, and be in mass ratio (1.5-5): 100 additive packages and basal liquid obtain
Etching solution；
S4, control etching solution temperature are 6-9 DEG C, are put into polysilicon chip, react 90-120S, obtain the silicon wafer that etching finishes.
In acid corrosion system, it is constant that the tension between each phase interface is determined by the property of silicon wafer itself, if reacting
Surfactant is added in system, then can reduce solution surface tension, to reduce infiltration angle, improves the wetting of silicon chip surface
Property, this means that the addition with surfactant, and the gas for reacting generation will quickly be detached from silicon face, to make polycrystalline
Silicon face is more uniform similar to pyramidal structure.
Polysilicon etch solution additive and its application of the invention has the advantages that compared with the existing technology
(1) additive of the invention can make reaction more steady after being added to etching reaction liquid, slow down reaction rate,
The reflectivity of the Reducing thickness of controllable silicon wafer and control silicon wafer simultaneously, more efficiently removal polysilicon chip are because of the machine that leaves after cutting
The impurity of tool damage and surface adhesion；
(2) it can be improved etching solution in the wetability of silicon face after additive of the invention is added in etching solution, make silicon
The bubble that piece surface generates during the reaction can be quickly detached from, so that polysilicon surface be made to form the erosion of structure more evenly
Carve hole.
Specific embodiment
Below in conjunction with embodiment of the present invention, the technical solution in embodiment of the present invention is carried out clearly and completely
Description, it is clear that described embodiment is only some embodiments of the invention, rather than whole embodiments.Base
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts all
Other embodiments shall fall within the protection scope of the present invention.
Embodiment 1
Mix 5g ethylene glycol monobutyl ether, 15g glucose, 100g sodium lactate, 2g vitamin C, 10g polyethylene glycol, 1g fluorine silicon
Sour sodium and 867g water control 120 DEG C, back flow reaction 8h, obtain etching solution additive；
The hydrofluoric acid of 100L40% mass concentration, the nitric acid and 200L water of 500L50% mass concentration are measured, is mixed
Uniformly, basal liquid is obtained；
15g etching solution additive and 1000g basal liquid are weighed, controlled at 6 DEG C, is uniformly mixed, is put into polysilicon chip,
90s is reacted, the silicon wafer that etching finishes is obtained.
Embodiment 2
Mix 20g ethylene glycol monobutyl ether, 30g glucose, 150g sodium lactate, 6g vitamin C, 40g polyethylene glycol, 8g fluorine silicon
Sour sodium and 746g water control 130 DEG C, back flow reaction 12h, obtain etching solution additive；
The hydrofluoric acid of 100L40% mass concentration, the nitric acid and 300L water of 600L50% mass concentration are measured, is mixed
Uniformly, basal liquid is obtained；
50g etching solution additive and 1000g basal liquid are weighed, controlled at 9 DEG C, is uniformly mixed, is put into polysilicon chip,
105s is reacted, the silicon wafer that etching finishes is obtained.
Embodiment 3
Mix 10g ethylene glycol monobutyl ether, 20g glucose, 130g sodium lactate, 4g vitamin C, 30g polyethylene glycol, 5g fluorine silicon
Sour sodium and 801g water control 125 DEG C, back flow reaction 10h, obtain etching solution additive；
The hydrofluoric acid of 100L40% mass concentration, the nitric acid and 400L water of 700L50% mass concentration are measured, is mixed
Uniformly, basal liquid is obtained；
30g etching solution additive and 1000g basal liquid are weighed, controlled at 7 DEG C, is uniformly mixed, is put into polysilicon chip,
120s is reacted, the silicon wafer that etching finishes is obtained.
Polysilicon etch solution additive of the invention is applied to wire cutting polycrystalline silicon texturing, gained making herbs into wool effect is such as
Under:
| Grouping | Additive-free etching | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Reflectivity/% | 24.47 | 19.24 | 19.33 | 19.27 |
| Open-circuit voltage/V | 0.6489 | 0.6642 | 0.6603 | 0.6642 |
| Short-circuit voltage/V | 8.3253 | 8.4284 | 8.5614 | 8.5023 |
| Reducing thickness/g | 0.42 | 0.34 | 0.25 | 0.28 |
The foregoing is merely better embodiments of the invention, are not intended to limit the invention, all of the invention
Within spirit and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of polysilicon etch solution additive, which is characterized in that including ethylene glycol monobutyl ether, glucose, sodium lactate, vitamin
C, polyethylene glycol, prodan and water.
2. a kind of polysilicon etch solution additive as described in claim 1, which is characterized in that be by mass percentage 100%
Meter, the ethylene glycol monobutyl ether are 0.5-2%, and the glucose is 1.5-3%, and the sodium lactate is 1-1.5%, the dimension life
Plain C is 0.2-0.6%, and the polyethylene glycol is 1-4%, and the prodan is 0.1-0.8%, and surplus is water.
3. a kind of polysilicon etch solution additive as described in claim 1, which is characterized in that the water is deionized water.
4. a kind of polysilicon etch solution additive as described in claim 1, which is characterized in that the molecular weight of the polyethylene glycol
For 500-2000.
5. the etching solution carved for polysilicon etching, which is characterized in that the etching solution includes polysilicon described in claim 1
The mass ratio of etching solution additive and basal liquid, the polysilicon etch solution additive and basal liquid is (1.5-5): 100.
6. the etching solution carved as claimed in claim 5 for polysilicon etching, which is characterized in that the basal liquid includes hydrogen fluorine
Acid, nitric acid and water, the hydrofluoric acid: nitric acid: the volume ratio of water is 1: (5-7): (2-4).
7. the etching solution carved as claimed in claim 6 for polysilicon etching, which is characterized in that the quality of the hydrofluoric acid is dense
Degree is 40%, and the mass concentration of the nitric acid is 50%.
8. a kind of method for carrying out acid etching using additive described in any one of Claims 1-4, which is characterized in that
Include the following steps:
It S1, is by mass percentage 100% meter, mixing 0.5-2% ethylene glycol monobutyl ether, 1.5-3% glucose, 1-1.5% cream
Sour sodium, 0.2-0.6% vitamin C, 1-4% polyethylene glycol, 0.1-0.8% prodan and surplus water, control temperature 120-
130 DEG C of back flow reaction 8-12h, obtain additive；
S2, be by volume 1: (5-7): (2-4) measures hydrofluoric acid, nitric acid and water, is mixed evenly, obtains basal liquid；
S3, control basal liquid temperature are at 6-9 DEG C, and be in mass ratio (1.5-5): 100 additive packages and basal liquid are etched
Liquid；
S4, control etching solution temperature are 6-9 DEG C, are put into polysilicon chip, react 90-120S, obtain the silicon wafer that etching finishes.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811547982.0A CN109554762B (en) | 2018-12-18 | 2018-12-18 | Polycrystalline silicon etching solution additive and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811547982.0A CN109554762B (en) | 2018-12-18 | 2018-12-18 | Polycrystalline silicon etching solution additive and application thereof |
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| Publication Number | Publication Date |
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| CN109554762B CN109554762B (en) | 2020-08-21 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111320982A (en) * | 2020-03-03 | 2020-06-23 | 苏州晶瑞化学股份有限公司 | Micro-etching rough treatment agent for wafer surface and treatment method thereof |
| CN113817472A (en) * | 2021-11-23 | 2021-12-21 | 绍兴拓邦电子科技有限公司 | Texturing process of solar cell silicon wafer |
| CN114214529A (en) * | 2020-09-04 | 2022-03-22 | 哈尔滨东盛金材科技股份有限公司 | Silicon additive for aluminum alloy smelting and preparation method thereof |
| CN116004232A (en) * | 2022-11-25 | 2023-04-25 | 常州君合科技股份有限公司 | Monocrystalline silicon polishing alkali etching additive and application thereof |
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